Apparatus for producing stannic chlorid.



PATENTED JAN. 21, 1908.

G. P. TOWNSEND.

R PRODUCING STANNIU CHLORID.

PP IOATION FILED 1 313.21, 1906.

APPARATU PATENTED JAN. 21, 1908.

C. P. TOWNSEND. APPARATUS FOR PRODUCING STANNIO GHLORID.

APPLICATION FILED FEB. 21, 1906.

Illlllll Z SHEETS-SHEET 2.

o Q m? e j Z2 W% f 4 UNIT D srn'rs ar rrrc.

I CLINTON PAUL TOWNSEND, OF WASHINGTON, DISTRICT OF COLUMBIA, ASSIGNORTO CHEMICAL REDUCTION COMPANY, OF-NEW YORK, N Y., A CORPORATION OF NEWYORK.

To all whom it may concern:

Be it known that I, CLINTON PAUL TOWN- SEND, a citizen of the UnitedStates, residing at Washington, in the District of Columbia, haveinvented certain new and useful Imrovements in I A paratus for Producingtannic.Chlorid, 0 which the following is a specification.

This invention is an apparatus for producin and recovering stannicchlorid from meta lic tin, or from any material which con tains tin inform capable of yielding a chlorid of tin by reaction with chlorin- Theapparatus is adapted to the recovery of stannic chlorid from. theproduct resulting from the detinnin of tin-scrap or cuttings, and willbe describe as a plied to such product by way of example. This productis commonly obtained as apowder containing from 80 to 95 per cent. of.tin, largely as metal, and relatively small proportions of lead andiron or their compounds.

Tin in this form can be refined and rendered marketable only atconsiderable cost, but is Well adapted to the production of stannicchlorid in the present apparatus. v

For a full understanding of the invention reference is made to theaccompanying drawigure 1 is aplan view of one form of apparatus Fig. 2is a side elevation of the'same range and Figs. 3 and 4 are details. v

Referring to the figures, reference numerals 110 represent a series ofvessels or retorts of which any desired or suitable number may be emloyed: these retorts are preferably ard in a continuous se ies with anumber of interposed condensers. The retorts shown constitute a seriesand are closely grouped, suitable means being provided for theapplication of heat as,.for instance, by embeddin all retorts in sand orother medium containe a pan indicated in outline by dotted lines 18,Figs. 1 and 2: heatis applied to this pan in any suitable way, as by thecontact of flue gases or the application of steam under suit- Theretorts may, of course, convenient means. The retorts are indicated asconsisting of acid proof stoneware. Each retort is provided with acentral aperture having a cover 19, this aperture serving for chargingthe retort and discharging the residuum; an

two lateral apertures 20, 21 for the passage of gases and vaporizedreactionproducts. The

able pressure.

Specification of Letters iatent. Application filed February 21. 1906-Serial No. 302121.8-

arrarus'ron ronuciu'e -s'raimrc cniionin.

Patented Jan. 21', lacs.

vessel or retort 1 communicates directly with illustrated comprising thepipes 22, 23 and the collecting vessels 1117. .It will be understoodthat in the production of stanni'c chlorid condensation occurs. also inthe exit pipe from the retort, and means for Withdrawing the liquid tromthis pipe may be used instead of the collecting vessels shown.

24 is a cock shown in detail in Figs. 3, 4. Chlorin is introducedthrough inlet 25, and is directed into either of the pipes 26 or 27 inaccordance with the position of the 0 ening'28 in the cap 29. When the000 is turned as illustrated in Fig. 3 the chlorin introduced at 25 willpass through pipe 26 into the vessel 1, thence in succession through theseveral retorts and interposed condensers, returning through pipe 27 tothe cock and'being directed by the tube 30, carried by the cap 29, tothe outlet 31 for waste gases. When the cock is revolved into theposition indicated in dotted lines in Fig. 3 the direction of flowthrough the retorts and condensers is reversed, the inlet and outletremaining unchanged. Any convenient means for controlling and reversingthe i'lOW of chlorin may be substituted. The pipes and collectingchambers constituting the condensers may, if desired, be rovided with aheat insulating cover. T e collecting chambers are conveniently ofglass, or other means are, provided for watching the progress of theoperation. The condenser pi es may advantageously extend for a consierable distance 4 into the retorts, as indicated-by dotted lines in Fig.2, whereby the current. of gas is directed toward the surface of thecharge.

In usin the above described apparatus the operatlon is conductedsubstantially as follows: The retorts 29 are char ed with thetin-bearing material, preferab y as a layer of relatively slight depth,and chlorin is admitted to the series, the chlorin being preferablyadmitted faster than it can be absorbed by the -tin in a single retort.The retorts are maintained during the distillation period at a suitabletemperature above the vaporizing point of stlannic chlo'ri'd (114 C),and the vaporized and entrained stannic chlorid together with the excessof chlorin passes into the condensing and collecting ap- 1t ls-necessarythat an excess of chlor1n be brought into presence of thetin; and thatstannic chlorid in a sin retort ordinarily paratus 2 2, 11, 23, theuncondensed portions passing thence to the retort 3 where a furtherbefore the distillation has begun in the last retort of the series.

For a clear understandin of the purgpose of the series arrangement ofretorts an interposed condensing means it should be understood that inorder to insure a rapid roduction and distillation of stannic chorid itis extremely difficult to secure a com lete condensation of'stannicchlorid, particu arly from a gas containing chlorin. It is clear,therefore, that if it be attempted to produce le retort followed by acondensing system, t ere will result a loss of chlorin representing theuncondensed portion. According to this invention such excess of chlorinas is desirable for rapid and economical production and distillation ofstannic chlorid is .used, and no particular necessity exists forproviding the complex apparatus which Wouldbe necessary for securing ana proximately com lete condensation of t e stannic chlori The gasespassing from the first condenser to the second contain both chlorin andstannic chlorid, both of which arerpuickly absorbedor condensed inpresenceo the tin in the second and following retorts. As each retort,in succession ceases to absorb chlorin and stannic chlorid it will beginthe delivery of stannic chlorid to its-condenser and the succeedingretorts. Before the last retort in series has ceased absorbing, one ormore of the retorts first in series Wlll have ceased distilling andshould then be recharged,

In the particular form of apparatus shown it is advisable at this sta eto reverse the direction of flow of chlorin through the'retorts byrotating the. cap 29 of the cock 24, permitting the chlorin to enter theretorts through pipe 27 and the waste gases to escape through ipe 26.The retorts 9, 8, 7, 6 will thenyidld stannic chlorid and the freshlycharged retorts 2, 3, 4, 5 will act as absorbers, stannic chlorid andthe number actin as absorbersfor the uncondensed gases wil of course,.bedependent uponthe total uantit be ore reversing the flow.

The apparatus may be so arranged as to obviate the necessity forreversing the flow of chlorin at intervalsz-for instance, the 'retortsmay be so connected that as the dist llation ceases in the first inseries, the chlorm is introduced into the second, the first The numberof retorts yielding of chlorin which has been intro uced erases beingre-charged and connected as an absorber at the end of the series.According to such arrangement the direct chlorin connection will betransferred successively to the retorts constituting the series.

The ap aratus as above described is suited for use with chlorin which isapproximately dry. If the chlorin contains considerable moistureitshould be dried, or, preferably, a

artor all of the contained molsture should e converted into hydrochloricacid. This is very conveniently effected as follows: The vessels 1 and10 are intended to contain por"- tions of the residue which remains inthe re- .torts 2-9 after the completion of the distillation. Thisresidue contains a considerable proportion of ferric chlorid, which,upon contact with wet chlorin at a suitable temperature, reacts with thecontained moisture to produce hydrochloric acid as follows This isadvantageous beoausethe reaction is accelerated by the presence ofhydrochloric acid, and also because that portion of the chlorin whichwould otherwise be lost as fer-- ric chlorid is recovered as stannicchlorid.

It is, of course, not essential that the vessels 1-10 for treating themoist chlorin should be grouped with the distilling retorts.

Instead of stoneware retorts, retorts of lead or of iron lined withlead, or such vessels as are employed as generators for chlorin by themanganese dio'xid method may be. 1

used.. I

If thechlorin be substantially undiluted a wide range of temperaturesabove the vaporizing point of stannic chlorid is applicable; if,however, the chlorin be diluted with a considerable proportion, of airsuch strong ignition as. wil result inoxidizing the tin should beavoided. I

The tin bearing material is preferably introduced in successive. smallcharges until the retorts are filled. The volume of the residue at theclose of the operation in case crude powder is treated equals or'exceeds that of the original charge, but its weight is, ofv course,relatively small. Its apparent specific gravity is thereforevery low andit may convenlently be discharged by a suction pipe introduced into thecentral aperture of.

the retort.

The heat developed by'the reaction between fresh bodies of tin andchlorin is fregluently sufficient to melt the tin, whereby ie retortsareendangeredi these may be protected by applying to the interior surface'a layer'of a suite e material such as asbestos aper, cement, etc.indicated at 32 in Fig. 2-

11 case the retorts are independently heated, heat will preferably beapplied only as re quired: during the earlystages of theabsor'p tron theapplication of heat is not necessary.

The process described herein isclaimed in-my copendingapplication,235,765, filed Dec. 6, 1904.

I claim v 1. In apparatus for producing stannic chlorid, a plurality ofnormally communicating retorts, means for supplying I chlorin thereto,and means for shifting the point of supply of chlorin.

'- 'ing chlorin, a; plurality of retorts arranged 'in series, condensingmeans interposed between said retorts, and means for conve ing chlorinsuccessively througlrsaid' dehy rating means and retorts.

4. In apparatus for producing stannic chlorid, in combinationmeans fordehydrating chlorin, a lurality of communicatlng retorts, means orconveying'chlorin through 'said' dehydrating means and retorts, .and

means for-shifting the point of supply of chlorin to said retorts 5. Inapparatus for producing stanhic chlorid, in combination means fordehydrating chlorin, a plurality of retorts arranged in series andconnected with said dehydrating 'means meansfor supplying chlorinthereto and means for shifting the point of supply of chlorin to saidretorts.

6. Apparatus'for producing stannic ch10 rld comprising n combinationmeans for dehydrating chlorin, a plurality of retorts varrangedin-series and connected-with said dehydrating means, means for supplyingchlorin thereto condensing means interposed between said retorts, andmeans for sh1fting the point of supply of chlorin to said retorts.

In testimony whereof, I afiix my signature,

in presence of two witnesses CLINTON PAUL TOWNSEND; Witnesses: l l

O. W. FOWILER, J. B, HILL.

